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Preparation method of vulcanization accelerator cz

A technology of vulcanization accelerator and accelerator, applied in the direction of organic chemistry, etc.

Inactive Publication Date: 2016-06-29
ZIBO GAOHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The key to the oxygen oxidation method is to choose a suitable catalyst with excellent performance. This method is still in the research stage in China.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] (1) beating into salt: take accelerator M167g, water 27g, cyclohexylamine 128.7g and copper acetate 0.15g for subsequent use; add water in the reactor, add accelerator M, cyclohexylamine and acetic acid under intense stirring Copper, so that the accelerator M and cyclohexylamine are fully beaten into salt;

[0077] (2) Oxidation: the temperature is raised to 40°C, and oxygen is introduced to make the pressure reach 0.35MPa, and the reaction is performed for 2h; then, the temperature is lowered, and sodium hypochlorite is added dropwise under the condition of 30°C to carry out the reaction, and the addition of sodium hypochlorite is stopped after the end point;

[0078] (3) suction filtration water washing: the suction filtration water washing product is neutral to obtain a white precipitate; the filtrate contains excessive cyclohexylamine, which is directly reused in the first step;

[0079] (4) Drying: The white precipitate is filtered, washed with water, dehydrated an...

Embodiment 2

[0081] (1) beating into salt: take accelerator M167g, water 30.6g, cyclohexylamine 168.3g and copper acetate 0.18g for subsequent use; add water in the reactor, add accelerator M, cyclohexylamine and Copper acetate, so that the accelerator M and cyclohexylamine are fully beaten into salt;

[0082] (2) Oxidation: the temperature is raised to 50°C, and oxygen is introduced to make the pressure reach 0.4MPa, and the reaction is performed for 4h; then, the temperature is lowered, and sodium hypochlorite is added dropwise for the reaction under the condition of 40°C, and the addition of sodium hypochlorite is stopped after the end point;

[0083] (3) suction filtration water washing: the suction filtration water washing product is neutral to obtain a white precipitate; the filtrate contains excessive cyclohexylamine, which is directly reused in the first step;

[0084] (4) Drying: The white precipitate is filtered, washed with water, dehydrated and dried, the drying temperature is ...

Embodiment 3

[0086] (1) beating into salt: take accelerator M167g, water 30g, cyclohexylamine 150g and copper acetate 0.16g for subsequent use; add water in the reactor, add accelerator M, cyclohexylamine and copper acetate under intense stirring , so that the accelerator M and cyclohexylamine are fully beaten into salt;

[0087] (2) Oxidation: the temperature was raised to 45°C, and oxygen was introduced to make the pressure reach 0.38MPa, and the reaction was performed for 3h; then the temperature was lowered, and sodium hypochlorite was added dropwise to react at 35°C, and the addition of sodium hypochlorite was stopped after reaching the end point;

[0088] (3) suction filtration water washing: the suction filtration water washing product is neutral to obtain a white precipitate; the filtrate contains excessive cyclohexylamine, which is directly reused in the first step;

[0089] (4) Drying: The white precipitate is filtered, washed with water, dehydrated and dried, the drying temperat...

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PUM

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Abstract

The invention belongs to the field of chemical synthesis technology, and particularly relates to a preparation method of a vulcanization accelerator CZ. The preparation method comprises the following steps: pulping and salifying, oxidizing, carrying out suction filtering and washing, and drying, thus obtaining the vulcanization accelerator CZ. By adopting a step-by-step oxidization method, namely a technology of oxygen oxidization at the earlier stage of the reaction and sodium hypochlorite oxidization at the later stage, the salt content of the waste water generated by adopting a sodium hypochlorite oxidization method can be effectively reduced, and the preparation method has the advantages of being simple in technology, low in cost, less in environment pollution and the like, thus being a green and environment-friendly technological route having industrial application values.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of a vulcanization accelerator CZ. Background technique [0002] At present, the production methods of accelerator CZ at home and abroad mainly include hydrogen peroxide oxidation, sodium hypochlorite oxidation, oxidant-free synthesis, and oxygen oxidation. [0003] (1) Hydrogen peroxide oxidation method [0004] The hydrogen peroxide oxidation method was successfully developed by the Czech Dimitrova Company in 1948. The synthesis method first put a certain amount of recovered cyclohexylamine into the reactor, and added 2 thiol benzothiazole (promoter M) under stirring. , add fresh cyclohexylamine and continue stirring to make M and cyclohexylamine fully miscible into a slurry. Then add hydrogen peroxide dropwise within a certain period of time, and the rate of addition ensures that the reaction temperature is below 30 ° C. After the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 蔡强蔡超蔡帅
Owner ZIBO GAOHUI CHEM
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